CN105271430B - A kind of preparation method of the ultra-dispersed ferroso-ferric oxide of modification - Google Patents

A kind of preparation method of the ultra-dispersed ferroso-ferric oxide of modification Download PDF

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CN105271430B
CN105271430B CN201510626184.7A CN201510626184A CN105271430B CN 105271430 B CN105271430 B CN 105271430B CN 201510626184 A CN201510626184 A CN 201510626184A CN 105271430 B CN105271430 B CN 105271430B
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ferriferrous oxide
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silane
dispersed
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CN105271430B8 (en
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李振宇
盛艳花
高力群
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Xuzhou Runfeng New Materials Co ltd
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JIANGSU ZHENYU ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
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Abstract

The invention discloses the preparation method of the ultra-dispersed ferroso-ferric oxide of a kind of modification, belong to ferroso-ferric oxide preparation field.The modified ultra-dispersed ferroso-ferric oxide of the present invention is iron chloride crystal and frerrous chloride crystal to be dissolved in deionized water, obtain iron ion mixed liquor, add NaOH intensification stirring reaction, separate, washing, it is dried to obtain nano ferriferrous oxide granule, then mix with ethanol solution, mix with methacryloxypropyl trimethoxy silane again, it is aged after temperature rising reflux, separating, washing obtains silane-modified ferriferrous oxide particles, add the dispersion of acetonitrile sonic oscillation, mix again modified with succinic acid, intensification high-speed stirred, cooling, filter, washing, it is dried, it is cooled to room temperature and obtains.The invention has the beneficial effects as follows: products therefrom of the present invention is difficult to reunite, and product component Modulatory character is strong, and crystal property and dispersive property are good;The method preparation is simple, and production process is pollution-free.

Description

A kind of preparation method of the ultra-dispersed ferroso-ferric oxide of modification
Technical field
The present invention relates to the preparation method of the ultra-dispersed ferroso-ferric oxide of a kind of modification, belong to ferroso-ferric oxide preparation field.
Background technology
Ferroso-ferric oxide, chemical formula Fe3O4, call iron oxide black, magnet, magnet, for having magnetic black crystals, therefore be also called magnetic iron oxide.It not the mixture of iron oxide and ferrous oxide, but the compound of ferrous oxide and iron oxide can be regarded approx as.This material is dissolved in acid, water insoluble, alkali and the organic solvent such as ethanol, ether.Natural ferroso-ferric oxide, insoluble in acid, is the most easily oxidized to di-iron trioxide under dampness.It is typically used as pigment and polishing agent it can also be used to manufacture audio tape and telecommunication apparatus.It addition, ferroso-ferric oxide or conductor, because due to Fe in magnetic iron ore2+With Fe3+Being substantially lack of alignment on octahedral site, electronics can shift rapidly between the two of iron kind oxidation state, so ferroso-ferric oxide solid has excellent electric conductivity.Ferroso-ferric oxide can be used for priming paint processed and finish paint, is to produce iron catalyst and the primary raw material of catalyst.Its hardness is very big, can make abrasive material.It is widely used to field of automobile brake, such as: brake block, brake shoe etc..Ferroso-ferric oxide field of welding material at home gets the nod, and the production for welding rod, welding wire still belongs to the starting stage, and market prospects are the most wide.Ferroso-ferric oxide is great because of its ratio, the feature that magnetic is strong, shows good performance in terms of sewage disposal.
Preparing ferroso-ferric oxide method at present and have coprecipitation, hydro-thermal method, mini-emulsion process and sol-gel process etc., wherein coprecipitation is the simplest, most economical synthetic method.Coprecipitation adds precipitating reagent in the solution containing multiple cation, allows all ions precipitate completely.In order to obtain uniform precipitation, generally it is slowly added to the salting liquid containing multiple cation in the precipitating reagent of excess be stirred, makes the concentration of all ions substantially exceed the equilibrium concentration of precipitation, make each component separate out as far as possible the most simultaneously.The ferriferrous oxide nano-particle that coprecipitation obtains mostly is spherical structure, and particle diameter is less is 5~10nm.But owing to the temperature ratio of this reaction is relatively low, so the crystallinity of the particle obtained is relatively poor.And, nanometer Fe prepared by this method3O4Particulate deposits is easily reunited between particle when washing, filtering and be dried, and course of reaction is complicated, and product is reunited and is seriously difficult to dispersion, and product component is difficult to regulate and control, and can affect nanometer Fe3O4Performance.
Summary of the invention
The technical problem to be solved: the nanometer Fe prepared for common coprecipitation3O4Particulate deposits is easily reunited between particle when washing, filtering and be dried, and course of reaction is complicated, and product is reunited and is seriously difficult to dispersion, and product component is difficult to regulate and control, and causes particle crystallization poor, Fe3O4The drawback that dispersiveness is poor, provide the preparation method of the ultra-dispersed ferroso-ferric oxide of a kind of modification, the present invention is by modified through silane, succinic acid twice by ferroso-ferric oxide, prepare the ferroso-ferric oxide of ultra-dispersed performance, the method preparation process is simple, products therefrom is difficult to reunite, and product component Modulatory character is strong, and crystal property and dispersive property are good.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) Fe is pressed2+And Fe3+Ion mol ratio is 1:1, chooses FeCl3•6H2O and FeCl2•4H2O is dissolved in deionized water, and under 650~750r/min rotating speeds, stirring makes it be completely dissolved subsequently, obtains iron ion mixed solution, presses Fe subsequently2+And OH-Mol ratio is 1:6, the sodium hydroxide solution of 1.3mol/L is joined in above-mentioned iron ion mixed solution, it is warming up at 50~60 DEG C, stirring reaction 1~2h, it is isolated with magnet after having reacted and washs 5~6 times with distilled water, it is placed in again at 60~70 DEG C and is dried 1~2h, prepare nano ferriferrous oxide granule;
(2) it is 1:3 by nano ferriferrous oxide and the ethanol solution mass ratio that mass fraction is 80%, nano ferriferrous oxide granule is added in ethanol solution, and the mixing that stirs at 20~30 DEG C, mixing speed is 600~800r/min, after it has stirred, it is 1:25 ratio in methacryloxypropyl trimethoxy silane and nano ferriferrous oxide mass ratio again, methacryloxypropyl trimethoxy silane is added in the mixed liquor that above-mentioned stirring completes, improving rotating speed is 1500~1800r/min, stirs 10~12h;
(3) after it has stirred, above-mentioned mixed liquor is warming up to 70~80 DEG C of backflows 1~2h, after its backflow terminates ageing 20~24h, it is drawn off being placed in a centrifuge centrifugation 10~15min, take lower sediment and wash 3~5 times with the ethanol solution that mass fraction is 80%, obtaining silane-modified ferriferrous oxide particles;
(4) above-mentioned prepared silane-modified ferriferrous oxide particles is taken, join equipped with in the beaker of the acetonitrile identical in quality with silane-modified ferriferrous oxide particles, and under 200~300W, sonic oscillation dispersion 10~20min, after its tentatively dispersion, mixed liquor 1:1 by volume after succinic acid and ultrasonic disperse is mixed, and it is warming up to 70~75 DEG C:
(5) after temperature reaches 70~75 DEG C, under the speed of 2600~2800r/min, high-speed stirred 20~24h, after it has stirred, mixed liquor is cooled to 60~65 DEG C, filters while hot, and ferriferrous oxide particles absolute ethyl alcohol and the distilled water after filtering washs 5~6 times respectively, being placed in the baking oven of 100~105 DEG C being dried 10~12h, dried taking-up naturally cools to room temperature, can be prepared by a kind of modified ultra-dispersed ferroso-ferric oxide.
Obtained by the present invention, modified ultra-dispersed ferroso-ferric oxide is black particle shape, and particle diameter is 10~20nm.
The present invention is compared with additive method, and Advantageous Effects is:
(1) products therefrom of the present invention is difficult to reunite, and product component Modulatory character is strong, and crystal property and dispersive property are good;
(2) the method preparation is simple, and production process is pollution-free.
Detailed description of the invention
First Fe is pressed2+And Fe3+Ion mol ratio is 1:1, chooses FeCl3•6H2O and FeCl2•4H2O is dissolved in deionized water, and under 650~750r/min rotating speeds, stirring makes it be completely dissolved subsequently, obtains iron ion mixed solution, presses Fe subsequently2+And OH-Mol ratio is 1:6, the sodium hydroxide solution of 1.3mol/L is joined in above-mentioned iron ion mixed solution, it is warming up at 50~60 DEG C, stirring reaction 1~2h, it is isolated with magnet after having reacted and washs 5~6 times with distilled water, it is placed in again at 60~70 DEG C and is dried 1~2h, prepare nano ferriferrous oxide granule;It is 1:3 by nano ferriferrous oxide and the ethanol solution mass ratio that mass fraction is 80% again, nano ferriferrous oxide granule is added in ethanol solution, and the mixing that stirs at 20~30 DEG C, mixing speed is 600~800r/min, after it has stirred, it is 1:25 ratio in methacryloxypropyl trimethoxy silane and nano ferriferrous oxide mass ratio again, methacryloxypropyl trimethoxy silane is added in the mixed liquor that above-mentioned stirring completes, improving rotating speed is 1500~1800r/min, stirs 10~12h;After it has stirred, above-mentioned mixed liquor is warming up to 70~80 DEG C of backflows 1~2h, after its backflow terminates ageing 20~24h, it is drawn off being placed in a centrifuge centrifugation 10~15min, take lower sediment and wash 3~5 times with the ethanol solution that mass fraction is 80%, obtaining silane-modified ferriferrous oxide particles;nullThen above-mentioned prepared silane-modified ferriferrous oxide particles is taken,Join equipped with in the beaker of the acetonitrile identical in quality with silane-modified ferriferrous oxide particles,And under 200~300W,Sonic oscillation dispersion 10~20min,After its tentatively dispersion,Mixed liquor 1:1 by volume after succinic acid and ultrasonic disperse is mixed,And it is warming up to 70~75 DEG C: finally after temperature reaches 70~75 DEG C,Under the speed of 2600~2800r/min,High-speed stirred 20~24h,After it has stirred,Mixed liquor is cooled to 60~65 DEG C,Filter while hot,And ferriferrous oxide particles absolute ethyl alcohol and the distilled water after filtering washs 5~6 times respectively,It is placed in the baking oven of 100~105 DEG C being dried 10~12h,Dried taking-up naturally cools to room temperature,Can be prepared by a kind of modified ultra-dispersed ferroso-ferric oxide.
Example 1
First Fe is pressed2+And Fe3+Ion mol ratio is 1:1, chooses FeCl3•6H2O and FeCl2•4H2O is dissolved in deionized water, and under 650r/min rotating speed, stirring makes it be completely dissolved subsequently, obtains iron ion mixed solution, presses Fe subsequently2+And OH-Mol ratio is 1:6, is joined by the sodium hydroxide solution of 1.3mol/L in above-mentioned iron ion mixed solution, is warming up to them at 50 DEG C, stirring reaction 1h, it is isolated with magnet after having reacted and washs 5 times with distilled water, then be placed at 60 DEG C dry 1h, prepare nano ferriferrous oxide granule;It is 1:3 by nano ferriferrous oxide and the ethanol solution mass ratio that mass fraction is 80% again, nano ferriferrous oxide granule is added in ethanol solution, and the mixing that stirs at 20 DEG C, mixing speed is 600r/min, after it has stirred, it is 1:25 ratio in methacryloxypropyl trimethoxy silane and nano ferriferrous oxide mass ratio again, methacryloxypropyl trimethoxy silane is added in the mixed liquor that above-mentioned stirring completes, raising rotating speed is 1500r/min, stirs 10h;After it has stirred, above-mentioned mixed liquor is warming up to 70 DEG C of backflow 1h, after its backflow terminates ageing 20h, is drawn off being placed in a centrifuge centrifugation 10min, take lower sediment and wash 3 times with the ethanol solution that mass fraction is 80%, obtaining silane-modified ferriferrous oxide particles;Then above-mentioned prepared silane-modified ferriferrous oxide particles is taken, join equipped with in the beaker of the acetonitrile identical in quality with silane-modified ferriferrous oxide particles, and under 200W, sonic oscillation dispersion 10min, after its tentatively dispersion, mixed liquor 1:1 by volume after succinic acid and ultrasonic disperse is mixed, and it is warming up to 70 DEG C: finally after temperature reaches 70 DEG C, under the speed of 2600r/min, high-speed stirred 20h, after it has stirred, mixed liquor is cooled to 60 DEG C, filter while hot, and ferriferrous oxide particles absolute ethyl alcohol and the distilled water after filtering washs 5 times respectively, it is placed in the baking oven of 100 DEG C being dried 10h, dried taking-up naturally cools to room temperature, can be prepared by a kind of modified ultra-dispersed ferroso-ferric oxide.
At a temperature of the obtained ultra-dispersed ferroso-ferric oxide of modification is placed in 200K, nano particle display superparamagnetism, saturation magnetization is 50emu/g, and without remanent magnetism, saturation magnetization is high, and product crystal property is preferable, and nano particle is uniformly dispersed, and dispersive property is good;When temperature is reduced to 10K, ferriferrous oxide nano-particle has magnetic trapping phenomena, and saturation magnetization increases to 60emu/g, and product is difficult to reunite and easily disperses, and product component Modulatory character is good, is worthy to be popularized and uses.
Example 2
First Fe is pressed2+And Fe3+Ion mol ratio is 1:1, chooses FeCl3•6H2O and FeCl2•4H2O is dissolved in deionized water, and under 700r/min rotating speed, stirring makes it be completely dissolved subsequently, obtains iron ion mixed solution, presses Fe subsequently2+And OH-Mol ratio is 1:6, is joined by the sodium hydroxide solution of 1.3mol/L in above-mentioned iron ion mixed solution, is warming up to them at 55 DEG C, stirring reaction 1.5h, it is isolated with magnet after having reacted and washs 6 times with distilled water, then be placed at 65 DEG C dry 1.5h, prepare nano ferriferrous oxide granule;It is 1:3 by nano ferriferrous oxide and the ethanol solution mass ratio that mass fraction is 80% again, nano ferriferrous oxide granule is added in ethanol solution, and the mixing that stirs at 25 DEG C, mixing speed is 700r/min, after it has stirred, then it is 1:25 ratio in methacryloxypropyl trimethoxy silane and nano ferriferrous oxide mass ratio, methacryloxypropyl trimethoxy silane is added in the mixed liquor that above-mentioned stirring completes, improve 1650r/min, stir 11h;After it has stirred, above-mentioned mixed liquor is warming up to 75 DEG C of backflow 1.5h, after its backflow terminates ageing 22h, is drawn off being placed in a centrifuge centrifugation 12min, take lower sediment and wash 4 times with the ethanol solution that mass fraction is 80%, obtaining silane-modified ferriferrous oxide particles;Then above-mentioned prepared silane-modified ferriferrous oxide particles is taken, join equipped with in the beaker of the acetonitrile identical in quality with silane-modified ferriferrous oxide particles, and under 250W, sonic oscillation dispersion 15min, after its tentatively dispersion, mixed liquor 1:1 by volume after succinic acid and ultrasonic disperse is mixed, and it is warming up to 72 DEG C: finally after temperature reaches 72 DEG C, under the speed of 2700r/min, high-speed stirred 22h, after it has stirred, mixed liquor is cooled to 62 DEG C, filter while hot, and ferriferrous oxide particles absolute ethyl alcohol and the distilled water after filtering washs 6 times respectively, it is placed in the baking oven of 103 DEG C being dried 11h, dried taking-up naturally cools to room temperature, can be prepared by a kind of modified ultra-dispersed ferroso-ferric oxide.
At a temperature of the obtained ultra-dispersed ferroso-ferric oxide of modification is placed in 250K, nano particle display superparamagnetism, saturation magnetization is 55emu/g, and without remanent magnetism, saturation magnetization is high, and product crystal property is preferable, and nano particle is uniformly dispersed, and dispersive property is good;When temperature is reduced to 15K, ferriferrous oxide nano-particle has magnetic trapping phenomena, and saturation magnetization increases to 65emu/g, and product is difficult to reunite and easily disperses, and product component Modulatory character is good, is worthy to be popularized and uses.
Example 3
First Fe is pressed2+And Fe3+Ion mol ratio is 1:1, chooses FeCl3•6H2O and FeCl2•4H2O is dissolved in deionized water, and under 750r/min rotating speed, stirring makes it be completely dissolved subsequently, obtains iron ion mixed solution, presses Fe subsequently2+And OH-Mol ratio is 1:6, is joined by the sodium hydroxide solution of 1.3mol/L in above-mentioned iron ion mixed solution, is warming up to them at 60 DEG C, stirring reaction 2h, it is isolated with magnet after having reacted and washs 6 times with distilled water, then be placed at 70 DEG C dry 2h, prepare nano ferriferrous oxide granule;It is 1:3 by nano ferriferrous oxide and the ethanol solution mass ratio that mass fraction is 80% again, nano ferriferrous oxide granule is added in ethanol solution, and the mixing that stirs at 30 DEG C, mixing speed is 800r/min, after it has stirred, it is 1:25 ratio in methacryloxypropyl trimethoxy silane and nano ferriferrous oxide mass ratio again, methacryloxypropyl trimethoxy silane is added in the mixed liquor that above-mentioned stirring completes, raising rotating speed is 1800r/min, stirs 12h;After it has stirred, above-mentioned mixed liquor is warming up to 80 DEG C of backflow 2h, after its backflow terminates ageing 24h, is drawn off being placed in a centrifuge centrifugation 15min, take lower sediment and wash 5 times with the ethanol solution that mass fraction is 80%, obtaining silane-modified ferriferrous oxide particles;Then above-mentioned prepared silane-modified ferriferrous oxide particles is taken, join equipped with in the beaker of the acetonitrile identical in quality with silane-modified ferriferrous oxide particles, and under 300W, sonic oscillation dispersion 20min, after its tentatively dispersion, mixed liquor 1:1 by volume after succinic acid and ultrasonic disperse is mixed, and it is warming up to 75 DEG C: finally after temperature reaches 75 DEG C, under the speed of 2800r/min, high-speed stirred 24h, after it has stirred, mixed liquor is cooled to 65 DEG C, filter while hot, and ferriferrous oxide particles absolute ethyl alcohol and the distilled water after filtering washs 6 times respectively, it is placed in the baking oven of 105 DEG C being dried 12h, dried taking-up naturally cools to room temperature, can be prepared by a kind of modified ultra-dispersed ferroso-ferric oxide.
At a temperature of the obtained ultra-dispersed ferroso-ferric oxide of modification is placed in 300K, nano particle display superparamagnetism, saturation magnetization is 60emu/g, and without remanent magnetism, saturation magnetization is high, and product crystal property is preferable, and nano particle is uniformly dispersed, and dispersive property is good;When temperature is reduced to 20K, ferriferrous oxide nano-particle has magnetic trapping phenomena, and saturation magnetization increases to 70emu/g, and product is difficult to reunite and easily disperses, and product component Modulatory character is good, is worthy to be popularized and uses.

Claims (1)

1. the preparation method of the ultra-dispersed ferroso-ferric oxide of modification, it is characterised in that concrete preparation process is:
(1) Fe is pressed2+And Fe3+Ion mol ratio is 1:1, chooses FeCl36H2O and FeCl24H2O is dissolved in deionized water, and under 650~750r/min rotating speeds, stirring makes it be completely dissolved subsequently, obtains iron ion mixed solution, presses Fe subsequently2+And OH-Mol ratio is 1:6, the sodium hydroxide solution of 1.3mol/L is joined in above-mentioned iron ion mixed solution, it is warming up at 50~60 DEG C, stirring reaction 1~2h, it is isolated with magnet after having reacted and washs 5~6 times with distilled water, it is placed in again at 60~70 DEG C and is dried 1~2h, prepare nano ferriferrous oxide granule;
(2) it is 1:3 by nano ferriferrous oxide and the ethanol solution mass ratio that mass fraction is 80%, nano ferriferrous oxide granule is added in ethanol solution, and the mixing that stirs at 20~30 DEG C, mixing speed is 600~800r/min, after it has stirred, it is 1:25 ratio in methacryloxypropyl trimethoxy silane and nano ferriferrous oxide mass ratio again, methacryloxypropyl trimethoxy silane is added in the mixed liquor that above-mentioned stirring completes, improving rotating speed is 1500~1800r/min, stirs 10~12h;
(3) after it has stirred, above-mentioned mixed liquor is warming up to 70~80 DEG C of backflows 1~2h, after its backflow terminates ageing 20~24h, it is drawn off being placed in a centrifuge centrifugation 10~15min, take lower sediment and wash 3~5 times with the ethanol solution that mass fraction is 80%, obtaining silane-modified ferriferrous oxide particles;
(4) above-mentioned prepared silane-modified ferriferrous oxide particles is taken, join equipped with in the beaker of the acetonitrile identical in quality with silane-modified ferriferrous oxide particles, and under 200~300W, sonic oscillation dispersion 10~20min, after its tentatively dispersion, mixed liquor 1:1 by volume after succinic acid and ultrasonic disperse is mixed, and it is warming up to 70~75 DEG C;
(5) after temperature reaches 70~75 DEG C, under the speed of 2600~2800r/min, high-speed stirred 20~24h, after it has stirred, mixed liquor is cooled to 60~65 DEG C, filters while hot, and ferriferrous oxide particles absolute ethyl alcohol and the distilled water after filtering washs 5~6 times respectively, being placed in the baking oven of 100~105 DEG C being dried 10~12h, dried taking-up naturally cools to room temperature, can be prepared by a kind of modified ultra-dispersed ferroso-ferric oxide.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101728047A (en) * 2010-01-25 2010-06-09 上海交通大学 Preparation method of ferroferric oxide magnetic nano particle emulsion
CN102108353A (en) * 2009-12-25 2011-06-29 华中科技大学 Magnetic nano-particle immobilized basic protease and preparation method and application thereof
CN102212162A (en) * 2011-03-25 2011-10-12 浙江大学宁波理工学院 Method for preparing thiolated nano ferroferric oxide magnetic polymer composite material
CN102225785A (en) * 2011-04-26 2011-10-26 东华大学 Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102108353A (en) * 2009-12-25 2011-06-29 华中科技大学 Magnetic nano-particle immobilized basic protease and preparation method and application thereof
CN101728047A (en) * 2010-01-25 2010-06-09 上海交通大学 Preparation method of ferroferric oxide magnetic nano particle emulsion
CN102212162A (en) * 2011-03-25 2011-10-12 浙江大学宁波理工学院 Method for preparing thiolated nano ferroferric oxide magnetic polymer composite material
CN102225785A (en) * 2011-04-26 2011-10-26 东华大学 Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles

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Address after: Jiangdong District 315000 Zhejiang city of Ningbo Province Yue Sheng Road No. 311 building 003 14-5

Patentee after: NINGBO JIANGDONG LINQING ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd.

Address before: Gaocheng town Gaocheng street Yixing city 213164 Jiangsu city of Changzhou Province

Patentee before: JIANGSU ZHENYU ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD.

C53 Correction of patent of invention or patent application
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Correction item: Patentee|Address

Correct: NINGBO JIANGDONG LINQING ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD.|Jiangdong District 315000 Zhejiang city of Ningbo Province Yue Sheng Road No. 311 building 003 14-5

False: Jiangsu Zhenyu EnvironmentaL Technology Co., Ltd.|Gaocheng town Gaocheng street Yixing city 213164 Jiangsu city of Changzhou Province

Number: 34

Volume: 32

CI03 Correction of invention patent

Correction item: Patentee|Address

Correct: NINGBO JIANGDONG LINQING ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD.|Jiangdong District 315000 Zhejiang city of Ningbo Province Yue Sheng Road No. 311 building 003 14-5

False: Jiangsu Zhenyu EnvironmentaL Technology Co., Ltd.|Gaocheng town Gaocheng street Yixing city 213164 Jiangsu city of Changzhou Province

Number: 34

Page: The title page

Volume: 32

ERR Gazette correction
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Inventor after: Ren Kangli

Inventor before: Li Zhenyu

Inventor before: Sheng Yanhua

Inventor before: Gao Liqun

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Address after: 300380 Tianjin city temple town Xiqing District Great Village days Building No. 27, No. 301 2

Patentee after: Ren Kangli

Address before: Jiangdong District 315000 Zhejiang city of Ningbo Province Yue Sheng Road No. 311 building 003 14-5

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Address before: 300380 Tianjin Xiqing District Dasi Town Darenzhuang Village Tianrenli 27 Building 2 Gate 301

Patentee before: Ren Kangli

Effective date of registration: 20181221

Address after: Room 11 409, Xuzhou Software Park, No. 6 Software Park Road, Quanshan District, Xuzhou City, Jiangsu Province, 221000

Patentee after: Chen Deyan

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Patentee before: BEIJING ZHITOUJIA INTELLECTUAL PROPERTY OPERATION CO.,LTD.

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